Process for flameproofing,waterproofing and oilproofing textile materials



United States Patent 3,441,433 PROCESS FOR FLAMEPROQFING, WATERPROOF- ING AND OILPRQOFING TEXTILE MATERIALS Claude Jean Michel, Senez, Chantilly, France, assignor to Ugine Kuhlmann, Paris, France No Drawing. Filed Dec. 24, 1964, Ser. No. 421,093 @laims priority, application France, Dec. 27, 1963,

8,664 Int. (:1. Dana /68, 11/00 US. Cl. 117-137 3 Claims ABSTRACT OF THE DISCLOSURE Process for flameproofing, waterproofing, and oilproofing cellulosic textile material comprising impregnating the material with an aqueous composition containing a phosphonitrile chloride and a polyfluoro aliphatic alcohol polyacrylate and heating.

or those obtained by the action of ammonia and methyl alcohol on phosphonitrile chlorides, give to cellulosic fibres a resistance to fire which is fast to repeated washing. Such fiameproofing substances are described, for example, in US. Patents Nos. 2,782,133 and 3,012,908 and in pending US. patent applications Ser. Nos. 281,057, 267,914, now US. Patent Number 3,193,571, and 366,184, now US. Patent Number 3,394,205. These substances will be referred to hereinafter as aminated flameprofing substances derived from phosphonitrile chlorides. The flameproofing treatment comprises, for example, impregnating fabrics with an aqueous solution of the flameproofing substance and subjecting the impregnated fabrics to a heat treatment to ensure fixation of the fiameproofing substance.

On the other hand, it is known that aqueous emulsions of polyfluoro derivatives impart to textile fibres the properties of resistance to water, oils, fats and solvents.

It has now been found that the fiameproofing substances mentioned above can be placed in a single bath with the aqueous emulsions of polyfluoro derivatives, and that the bath so prepared, having good stability, confers on textile materials impregnated therein and then subjected to a heat treatment, flameproofing, waterproofing and oilproofing properties which have an excellent resistance to washing.

According to the present invention a process for flame proofing, waterproofing and oilproofing of cellulosic textile materials, is provided which comprises impregnating the material in an aqueous bath containing an aminated fiameproofing substance derived from a phosphonitrile chloride and an aqueous emulsion of a polyfluoro derivative, and subjecting the impregnated textile material to a heat treatment.

The temperature of the heat treatment is advantageously between 120 C. and 230 C. and its duration, which varies inversely with the temperature, may be as short as seconds at 230 C. but as long as one hour at a lower temperature.

The quantity of fiameproofing substance and polyfluoro derivative to be used depends on the degree of resistance to washing that is desired.

"ice The invention also includes the novel aqueous treatment baths containing an aminated flameproofing substance and an aqueous emulsion of a polyfluoro derivative.

The aqueous treatment bath may contain in addition to the fiameproofing substance and the polyfluoro derivative, any products intended to improve the flameproofing or to bring about other effects, for example antifungal or crease-resisting effects.

The invention further includes cellulosic textile material rendered fiameproof, waterproof and oilproof by the process of the invention.

The aqueous emulsion of polyfluoro derivatives which may be used for carrying out theinvention may be, for example, a latex of polyfluoro aliphatic alcohol polyacrylates, such as those mentioned in the Textile Research Journal, vol. 32 (April 1962), pages 320 to 331, or those marketed by the Minnesota Mining and Manufacturing Co., under the name of Scotchgard.

The aminated fiameproofing substances derived from phosphonitrile chlorides fix the polyfluoro derivatives on the fibres and give them fastness to repeated washing at the boil, which property they did not previously have, while these same fiuoro derivatives only alter very slightly the permanence of the fiameproofing. In addition, the presence of the polyfluoro derivative substantially permanently protects the resistance to tearing of the fabrics and keeps it equal to that of the nonflameproofed fabric.

The following examples in which the proportions are by weight, are purely illustrative.

Example 1 An aqueous bath is prepared containing 25% of the aminated flameproofing substance described in Example 1 of US. patent application Ser. No. 267,914, 5% of urea, 5% of an emulsion of polyfluoro derivative known on the market by the name of Scotchgard stain repeller PC 208. A cotton satin fabric, well boiled, and if desired bleached, weighing 300 g. to the square metre, is padded in this bath so that the squeezing rate is it is dried, exposed for 5 minutes to a temperature of C., rinsed and again dried. A fabric is obtained the resistance to tearing of which is unaltered after 10 washes and the waterproofing, fiameproofing and oilproofing properties of which are still satisfactory after 10 washes. These washes are carried out at the boil in a bath containing, per litre, 5 g. of Marseilles soap and 2 g. of sodium carbonate.

Example 2 An aqueous bath is prepared containing 25% of the aminated flameproofing substance described in Example 5 of the US. Patent 3,012,908, 5% of urea, 3% of an emulsion of the polyfluoro derivative known on the market by the name of Scotchgard stain repeller PC 208. In this bath a well-boiled cotton twill fabric, weighing 330 g. to the square metre, is padded so that the squeezing rate is 80%; the fabric is dried, fixed for 5 minutes at 150 C., rinsed and again dried. A fabric is obtained the resistance to tearing of which is unaltered after 10 washes and the Waterproofing, fiameproofiing and oil-proofing properties of which are still satisfactory after 10 washes. These washes are carried out at the boil in a bath containing 5 g. of Marseilles soap and 2 g. of sodium carbonate per litre.

Example 3 An aqueous bath is prepared containing 30% of the aminated flameproofing substance described in Example 5 of US. Patent 3,012,908, 6% of urea and 3% of an emulsion of the polyfluoro derivative known on the market by the name of Scotchgard sain repeller PC 210. In this bath a Well-boiled cotton twill fabric, weighing 280 g. to the square metre, is padded so that the squeezing rate is 3 80%. The fabric is dried, fixed for 5 minutes at 155 C., rinsed in water at 60 C. and again dried. A fabric is obtained the waterproofing, fiarneproofing and oilproofing properties of which are still satisfactory after Washes.

Example 4 An aqueous bath is prepared containing 30% of the aminated flame-proofing substance described in Example 1 of U5. patent application Ser. No. 267,914, 6% of urea and 4% of an emulsion of the polyfiuoro derivative known on the market by the name of Scotchgard stain repeller PC 208. In this bath a cotton gabardine fabric, previously boiled, mercerized and dyed with vat dyes, is padded so that the squeezing rate is 80%; the fabric is dried, fixed for 5 minutes at 155 C., rinsed in water at 60 C. and again dried. A fabric is obtained the waterproofing, flameproofing and oilproofing properties of which are still satisfactory after 10 washes of minutes each in a bath at 60 C. containing, per litre, 5 g. of Marseilles soap and 2 g. of sodium carbonate.

In place of the flameproofing substances of the above examples one may use any of the flameproofing substances described and claimed in the above-mentioned U.S. patents and pending US. patent applications.

I claim:

1. Process for the flameproofing, waterproofing and oilproofing of cellulosic textile material which comprises impregnating the material in an aqueous bath containing as the essential ingredients an aminated fiameproofing substance derived from a phosphonitrile chloride and a waterproofing and oilproofing substance consisting of at least three percent (3%) of an aqueous emulsion of a polyfiuoro aliphatic alcohol polyacrylate, and subjecting the impregnated textile material to a heat treatment.

2. Process according to claim 1 wherein the temperature of the heat treatment is between C. and 230 C.

3. Process according to claim 1 wherein the duration of the heat treatment is from some seconds to one hour.

References Cited UNITED STATES PATENTS 2,642,416 6/1953 Ahlbrecht et al 1l7-l36 2,782,133 2/1957 Vallette 1l7138 3,012,908 12/1961 Bilger 2528.1 3,193,571 7/1965 Bilger 2528.1 3,304,198 2/1967 Woolf 117-143 WILLIAM D. MARTIN, Primary Examiner.

H. J. GWINNELL, Assistant Examiner.

US. Cl. X.R. 

